本文采用固相烧结法制备了ZrV2-xPxO7@=0,0.2,0.4,0.6,0.8,1)系列材料.粉末X射线衍射(XRD)分析表明,所制备材料的结构为单一立方相.应用变温拉曼光谱研究该材料相变,变温拉曼光谱研究结果表明,材料起始相变温度随着P5+替代V5+量的增加逐渐降低,x=0,0.4,0.8,1对应的相变温度分别为383K,363K,273K,213K.热膨胀测试结果表明:随着P替代量的增加正一负膨胀转变温度先降低后增加,x=0,0.2,0.4,0.6,0.8,1对应的正一负膨胀转变温度分别为429K,403K,372K,390K,398K和435K.本文指出了该系列材料存在两个相变过程,为设计和制备ZrV2O7基室温附近的负热膨胀材料奠定了良好的基础.
ZrV2-xPxO7 (x = 0, 0.4, 0.8, 1.0) solid solutions are prepared using a solid state reaction method. Powder X-ray diffraction (XRD) analysis reveals that the as-prepared solid solutions are of single-phase cubic type in crystal structure. Temperature dependent Raman spectroscopic studies demonstrate that the phase transition temperature of ZrV2-xPxO7 decreases with the increase of the content of P. ZrV2O7, ZrV1.6P0.4O7, ZrV1.2P0.8O7 and ZrVPO7 transform from a 3 × 3 ×3 superstructure to a 1 ×1 × 1 normal structure at about 373 K, 363 K 273 K and 213 K, respectively. The results of thermal expansion testing indicate that the temperature of positive thermal expansion changes to negative thermal expansion with the increase of P content. The temperatures of positive-to- negative thermal expansion of ZrV2-xPxO7 are 429 K, 403 K, 372 K, 390 K, 398 K and 435 K for x = 0, 0.2, 0.4, 0.6, 0.8 and 1, respectively. Two phase change transformations are demonstrated in ZrV2-xPxO7 materials in our work, which is beneficial for preparing the negative thermal expansion materials at room temperature using ZrV2 07.